CN103614146B - Polymer dispersed liquid crystal material, display apparatus containing same and preparation method thereof - Google Patents
Polymer dispersed liquid crystal material, display apparatus containing same and preparation method thereof Download PDFInfo
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- CN103614146B CN103614146B CN201310626216.4A CN201310626216A CN103614146B CN 103614146 B CN103614146 B CN 103614146B CN 201310626216 A CN201310626216 A CN 201310626216A CN 103614146 B CN103614146 B CN 103614146B
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Abstract
The invention relates to a polymer dispersed liquid crystal (PDLC) material which is low in voltage and wide in temperature mode, wherein the material consists of a liquid crystal material, an aliphatic polyurethane acrylate oligomer, an acrylate monomer, a photoinitiator and interstitials. The invention further provides a polymer dispersed liquid crystal display apparatus prepared by using the polymer dispersed liquid crystal material and a preparation method thereof. The polymer dispersed liquid crystal material provided by the invention has the advantages of wide raw material source and simple and convenient preparation process. The PDLC display apparatus prepared from the PDLC material has the advantages of low driving voltage, wide range of working temperature, no shrinkage and deformation and good adhesive force. The preparation method of the PDLC display apparatus is simple and convenient, the thickness of the display apparatus can be adjusted according to size of the interstitials added, and the display apparatus obtained is good in adhesive force and not easy to shrink and deform, so that the PDLC display apparatus with a large area can be probably prepared.
Description
Technical field
The present invention relates to liquid crystal material and liquid crystal display device field, be specifically related to a kind of low-voltage, wide temperature range type polymer dispersion liquid crystal material, polymer dispersed liquid crystal display part and preparation method thereof by described polymer dispersion liquid crystal material gained.
Background technology
Polymer Dispersed Liquid Crystal (Polymer Dispersed Liquid Crystal, PDLC) be a kind of compound liquid-crystal material with special photoelectric properties, its principle is after small molecule liquid crystal material and polymer mixed, polymkeric substance issues looks at external influence and is separated, and liquid crystal molecule scatter to be formed and has display or light modulation effect from potpourri.Existing technology initiation conditions is mainly heat and causes and ultraviolet light (UV) initiation.
PDLC display device is without in external electric field situation, and in different droplet, the sensing of the director of liquid crystal is random, and thus PDLC display device presents the strong scattering process of light, presents milky; If apply certain electric field, be enough to make all liquid crystal droplet directors and field parallel, if the ordinary refraction index of liquid crystal is consistent with refractive index polymer, then PDLC presents pellucidity.PDLC display device and conventional liquid crystal have many different: its structure does not simply need polaroid IC module, does not need strict control to two substrates spacing, to production environment and liquid crystal quality requirements lower, its film thickness can according to spacer size free adjustment.
At present, pdlc film mainly with glass or mylar for substrate base material, because its raw material sources are extensive, unique photoelectric properties, manufacture craft is simple, and the advantages such as cost is lower, are widely used in optoelectronic switch, projector, intelligent glass, grating etc.But these application also exist driving voltage higher, easily influenced by ambient temperature, easy cracking the weak point such as to come unstuck, make it be restricted in application aspect.
Summary of the invention
For the voltage overcoming existing pdlc film is high, technological deficiency easily influenced by ambient temperature, the object of this invention is to provide Polymer Dispersed Liquid Crystal (PDLC) material of a kind of low-voltage, wide temperature range type.
The technical scheme realizing the object of the invention is:
A kind of polymer dispersion liquid crystal material, consists of the following composition by weight:
Liquid crystal material: 30 ~ 80 parts;
Aliphatic urethane acrylate oligomer: 5 ~ 30 parts;
Acrylate diluting monomer: 10 ~ 30 parts;
Light trigger: 1 ~ 8 part;
Spacer: 0.1 ~ 2 part;
Wherein, described liquid crystal material is Nematic phase liquid crystal material.
Preferably, described polymer dispersion liquid crystal material consists of the following composition by weight:
Liquid crystal material: 45 ~ 65;
Aliphatic urethane acrylate oligomer: 15 ~ 30;
Acrylate diluting monomer: 15 ~ 30;
Light trigger: 1 ~ 5;
Spacer: 0.1 ~ 2;
Wherein, described liquid crystal material is Nematic phase liquid crystal material, and wherein the structure of liquid crystal material is made up of following compound mixing:
Wherein, R
1, R
2, R
3, R
4be respectively the alkyl of 1-3 C atom, L
1, L
2, L
3, L
4be respectively-CN or-F.
Four kinds of compounds can be any proportioning.Preferably, in described liquid crystal material, the weight portion of formula (I) compound is 13-32 part, and the weight portion of formula (II) compound is 6-27 part, and formula (III) compound by weight part is 22-48 part, and formula (IV) compound by weight part is 6-20 part.
Preferably, the optical parametric of described Nematic phase liquid crystal material is: cleaning point is greater than 100 DEG C, Δ ε >=12.0, and Δ n >=0.20, no is between 1.50 ~ 1.52.Such as Bayi Space produces BNHR series liquid crystal material.
Wherein, described aliphatic urethane acrylate oligomer viscosities is 3000 ~ 8000cps; Described diluting monomer is one or more in ethoxyethoxyethyl acrylate, 2-ethylhexyl acrylate, β-hydroxyethyl methacry-late, hydroxy propyl methacrylate, isobornyl methacrylate, 1,6-hexanediyl ester, trimethylolpropane triacrylate, trimethylolpropane tris (3-mercaptopropionic acid ester), tetramethylol methane tetraacrylate; Three kinds in preferred described monomer or four kinds.Three kinds or four kinds of monomers are combined and can regulate driving voltage and adhesion, and regulate ratio to adapt to the preparation technology of product, after UV solidification, show better combination property.
Described light trigger is one or more in 1-hydroxycyclohexyl phenyl ketone (184), benzoin dimethylether (651), 2-hydroxy-2-methyl-1-phenyl-1-acetone (1173).
A kind of polymer dispersed liquid crystal display part, comprise and be coated with the upper and lower substrate of conductive layer and the polymer dispersed liquid crystal film between two substrates respectively, described upper and lower base plate is mylar or glass material, and described polymer dispersed liquid crystal film is that polymer dispersion liquid crystal material of the present invention solidification obtains.
Wherein, the spacing of described upper and lower substrate is determined by light-transmitting gap, and its size is 12 ~ 20 μm; The conductive layer that upper and lower substrate is coated with is selected from ITO(tin indium oxide), FTO(fluorine oxide tin), ZTO(zinc-tin oxide) one in conductive layer.
The preparation method of polymer dispersed liquid crystal display part of the present invention, comprises the following steps:
(1) liquid crystal material, aliphatic urethane acrylate oligomer, acrylate diluting monomer, light trigger and spacer are mixed to it for clear solution;
(2) clear solution of step (1) gained is coated in is coated with between conductive layer two substrates;
(3) two substrates after step (2) process is fixed the solderless substrate of thickness through running roller pressing;
(4) gained solderless substrate is carried out ultraviolet light polymerization, obtain described polymer dispersed liquid crystal display part.
Wherein, the described clear solution of step (2) adopts rolling method, knife coating or curtain coating to be coated between two substrates, selects roller coat or blade coating, select roller coat or showering when substrate used thereof material is mylar when substrate used thereof material is glass material.
Be coated with the upper and lower substrate of conductive layer, require that described glass or mylar base material resistance are 130 ~ 400 Ω, transmitance >=85, mist degree < 3, wherein the thickness of mylar is 125 ~ 200 μm, and hardness is >=3.
Wherein, the ultraviolet wavelength of step (4) described ultraviolet light polymerization is 250 ~ 380nm, intensity is 10 ~ 30mW/cm
2; The time of solidification is 2 ~ 10 minutes, temperature is 40 ~ 70 DEG C.
In above-mentioned preparation method, described pressing, ultraviolet light polymerization adopt the existing technology in this area and equipment can realize, as conventional pressing machine, ultraviolet curing lamp etc.
Beneficial effect of the present invention is:
PDLC material provided by the invention has that raw material sources are extensive, preparation technology is easy, and the PDLC display device adopting described PDLC material to make has the advantage that driving voltage is low, operating temperature range is wide, do not shrink indeformable stable performance.
PDLC display device provided by the invention makes large area display by splicing, is applied to the public arenas such as station, airport, school, theater and plays a role in fields such as house ornamentation, office and instrument and meters, having heavy industrialization application prospect.
Accompanying drawing explanation
Fig. 1 is the sectional structure chart of PDLC display device perpendicular to orientation substrate;
Fig. 2 is the preparation flow figure of PDLC display device;
Fig. 3 is the V-T curve of the PDLC display device that embodiment 1 material makes, and wherein, horizontal ordinate is voltage (V), ordinate is transmitance (%).
Fig. 4 is temperature-contrast and the temperature-voltage curve of the PDLC display device that embodiment 1 material makes, and wherein, horizontal ordinate is temperature (T), ordinate is respectively contrast and voltage (V).
In figure, 1, upper substrate base material; 2, upper substrate conductive layer; 3, spacer; 4, infrabasal plate conductive layer; 5, infrabasal plate base material.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Raw material used in the present invention is as follows: oligomer is that Yantai cloud becomes civilized the aliphatic urethane acrylate (viscosity (60 DEG C): 3000-8000cps) of YKDBA-01 series of work responsibility company limited.
The BNHR series mixed liquid crystal product that liquid crystal material uses Beijing Bayi Space liquid crystal Science and Technology Ltd. to provide, weight portion 13-32 part of its Chinese style (I) compound, weight portion 6-27 part of formula (II) compound, formula (III) compound by weight part 22-48 part, formula (IV) compound by weight part 6-20 part, mixes.Its parameter is: cleaning point >100 DEG C, Δ ε >=12.0, and Δ n >=0.20, no is between 1.50 ~ 1.52.
Be coated with the substrate of ITO conductive layer purchased from Yu Xing glass material company limited of Shenzhen.
Spacer is the product of 12 ~ 20 μm of different sizes of Shenzhen Na Wei Science and Technology Ltd..
Acrylate diluting monomer is common commercial reagent, but is not limited thereto.
Except specified otherwise, in embodiment, the content of each component all represents mass percent.
Embodiment 1
Polymer dispersion liquid crystal material component described in the present embodiment and formula are in table 1.
Table 1: embodiment 1 component
Embodiment 2
Polymer dispersion liquid crystal material component described in the present embodiment and formula are in table 2.
Table 2: embodiment 2 component
Embodiment 3
Polymer dispersion liquid crystal material component described in the present embodiment and formula are in table 3.
Table 3: embodiment 3 component
Embodiment 4
Polymer dispersion liquid crystal material component described in the present embodiment and formula are in table 4.
Table 4: embodiment 4 component
Embodiment 5
Material in polymer dispersion liquid crystal material employing embodiment 1 and formula, take altogether 10g PDLC material.
The preparation process of PDLC display device comprises the following steps (see Fig. 2):
Step 1: get one, clean 50ml beaker, 2.00g aliphatic urethane acrylate YKDBA-01-III, 1.00g trimethylolpropane tris (3-mercaptopropionic acid ester), 0.50g1,6-hexanediyl ester, 0.45g2-ethylhexyl acrylate, 1.00g β-hydroxyethyl methacry-late, 4.70g BNHR40600 liquid crystal material, 0.30g light trigger and 0.05g spacer (20 μm) is added successively in beaker.Then adding stirring magneton in the mixture, put into by beaker on magnetic stirring apparatus, stirring at room temperature 15-20 minute, is clear solution to mixed liquor.Lucifuge is noted in weighing, whipping process.
Step 2: the method for PDLC material roller coat step 1 obtained evenly is coated in and is coated with between ITO conductive layer two substrates.
Step 3: by the two substrates pressing machine pressing scribbling PDLC material of gained.
Step 4: the substrate after pressing is put into UV lamp box and solidifies, solidification wavelength is mainly 365nm, and solidification intensity is 20mW/cm
2, solidification temperature is 50 DEG C, and set time is 3min.
Can obtain PDLC display device by above step, as shown in Figure 1, the thickness of (wherein PDLC material does not draw) its PDLC material layer is 20 μm.The upper and lower substrate 1,5 being coated with ITO conductive layer 2,4 is glass baseplate, and the resistance (sheet resistance) of ito substrate is 130 ~ 400 Ω, transmitance >=85, mist degree < 3.The spacing of upper and lower substrate is determined by light-transmitting gap, and its size is 20 μm.As shown in Figure 3, the curve of its temperature and contrast, voltage as shown in Figure 4 for this PDLC display device transmitance-voltage (V-T) curve (room temperature).As seen from Figure 3, the driving voltage of PDLC display device is lower, and the driving voltage when transmitance is 70% only has about 15v.As seen from Figure 4, the temperature dependency of PDLC display device is better, and along with the change of temperature variation contrast is less, and voltage varies with temperature also in a little scope.
Embodiment 6
Material in polymer dispersion liquid crystal material employing embodiment 2 and formula, take altogether 10g PDLC material.
The preparation process of PDLC display device comprises the following steps:
Step 1: get one, clean 50ml beaker, adds 1.80g aliphatic urethane acrylate YKDBA-01-VI, 0.30g trimethylolpropane triacrylate, 0.80g hydroxy propyl methacrylate, 0.20g isobornyl methacrylate, 1.15g ethoxyethoxyethyl acrylate, 5.40g BNHR40500 liquid crystal material, 0.30g light trigger D1173 and 0.05g spacer (14 μm) successively in beaker.Then adding stirring magneton in the mixture, put into by beaker on magnetic stirring apparatus, stirring at room temperature 15-20 minute, is clear solution to mixed liquor.Lucifuge is noted in weighing, whipping process.
Step 2: the method for PDLC material showering step 1 obtained evenly is coated in and is coated with between ITO conductive layer two substrates.
Step 3: by the two substrates pressing machine pressing scribbling PDLC material of gained.
Step 4: the substrate after pressing is put into UV lamp box and solidifies, solidification wavelength is mainly 365nm, and solidification intensity is 30mW/cm
2, solidification temperature is 55 DEG C, and set time is 2min.
Wherein, step 2 and step 3 can be carried out simultaneously.
Can obtain PDLC display device by above step, the thickness of its PDLC material layer is 14 μm, and driving voltage is low, and the driving voltage when transmitance is 70% is at about 10v, and contrast is good.
Embodiment 7
The substrate being coated with ITO conductive layer is mylar material, and resistance is 200 ~ 300 Ω, transmitance >=85, mist degree < 3, and thickness is 125 ~ 200 μm, and hardness is >=3.Other materials adopts material and the formula of embodiment 3,4 respectively, and preparation method of the present invention prepares display device.Its result and embodiment 5,6 similar, the driving voltage of PDLC display device is lower, and the driving voltage when transmitance is 70% is between 10-20v, and contrast is good.
Above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various modification that the common engineering technical personnel in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (4)
1. a polymer dispersed liquid crystal display part, comprise and be coated with the upper and lower substrate of conductive layer and the polymer dispersed liquid crystal film between two substrates respectively, described upper and lower base plate is mylar or glass material, described polymer dispersed liquid crystal film is that polymer dispersion liquid crystal material solidification obtains, it is characterized in that
The spacing of described upper and lower substrate is 12 ~ 20 μm; The conductive layer that upper and lower substrate is coated with is selected from the one in ITO, FTO, ZTO conductive layer;
Described polymer dispersion liquid crystal material, consists of the following composition by weight:
Liquid crystal material: 45 ~ 65;
Aliphatic urethane acrylate oligomer: 15 ~ 30;
Acrylate diluting monomer: 24.5 ~ 29.5;
Light trigger: 1 ~ 5;
Spacer: 0.1 ~ 2;
Wherein the structure of liquid crystal material is made up of following compound mixing:
Wherein, R
1, R
2, R
3, R
4be respectively the alkyl of 1-3 C atom, L
1, L
2, L
3, L
4be respectively-CN or-F;
In described liquid crystal material, the weight portion of formula (I) compound is 13-32 part, the weight portion of formula (II) compound is 6-27 part, and formula (III) compound by weight part is 22-48 part, and formula (IV) compound by weight part is 6-20 part;
Wherein, described aliphatic urethane acrylate oligomer viscosities is 3000 ~ 8000cps; Described diluting monomer is one or more in ethoxyethoxyethyl acrylate, 2-ethylhexyl acrylate, β-hydroxyethyl methacry-late, hydroxy propyl methacrylate, isobornyl methacrylate, 1,6-hexanediyl ester, trimethylolpropane triacrylate, trimethylolpropane tris (3-mercaptopropionic acid ester), tetramethylol methane tetraacrylate; Described light trigger is one or more in 1-hydroxycyclohexyl phenyl ketone (184), benzoin dimethylether (651), 2-hydroxy-2-methyl-1-phenyl-1-acetone (1173).
2. polymer dispersed liquid crystal display part according to claim 1, is characterized in that, is obtained by following preparation method:
(1) liquid crystal material, aliphatic urethane acrylate oligomer, acrylate diluting monomer, light trigger and spacer are mixed to it for clear solution;
(2) clear solution of step (1) gained is coated in is coated with between conductive layer two substrates;
(3) two substrates after step (2) process is fixed the solderless substrate of thickness through running roller pressing;
(4) gained solderless substrate is carried out ultraviolet light polymerization, obtain described polymer dispersed liquid crystal display part.
3. polymer dispersed liquid crystal display part according to claim 2, it is characterized in that, the described clear solution of step (2) of preparation method adopts rolling method, knife coating or curtain coating to be coated between two substrates, select roller coat or blade coating when substrate used thereof material is glass material, when substrate used thereof material is mylar, select roller coat or showering.
4. the polymer dispersed liquid crystal display part according to Claims 2 or 3, is characterized in that, the ultraviolet wavelength of step (4) the described ultraviolet light polymerization of preparation method is 250 ~ 380nm, intensity is 10 ~ 30mW/cm
2; The time of solidification is 2 ~ 10 minutes, temperature is 40 ~ 70 DEG C.
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